反应详情

To a stirred solution of 1-(4-ethoxyphenyl)-2,2,3,3-tetrafluorocyclobutane carbonyl chloride (0.76 gm, 1.54 mmole) in dry benzene (10 ml) was added a solution of 2-hydroxymethyl-6-phenoxypyridine (0.305 g) and pyridine (0.12 g) in dry benzene (15 ml). The mixture was stirred at room temperature for 16 hours then diluted with ether, washed twice with water, dried over Na2SO4 and concentrated in vacuo. Purification by high pressure liquid chromatography gave the ester as a colourless oil. IR (film) λmax 1741, 1606, 1591, 1575, 1500, 1490, 1450 cm-1. N.m.r. (250 MHz) δ (CDCl3) 1.42, t, 3H, J=7 Hz, CH3 ; 2.90-3.08, m, 1H, cyclobutyl H; 3.44-3.64, m, 1H, cyclobutyl H; 4.02, q, 2H, J=7 Hz, CH2CH3 ; 5.10, 5.16, ABq, 2H, J=14.5 Hz, CH2 -O; 6.71-7.64, m, 13H, aromatic H's. Mass spectrum, m/z 476 (M+ +1), 456 (M+ -19).

1. washwashed twice with water
2. dry with materialdried over Na2SO4
3. concentrationconcentrated in vacuo
4. customPurification by high pressure liquid chromatography